CN112778950A - Efficient intermediate-temperature fast-curing epoxy structural adhesive for die assembly and bonding of wind power generation blades and preparation method thereof - Google Patents
Efficient intermediate-temperature fast-curing epoxy structural adhesive for die assembly and bonding of wind power generation blades and preparation method thereof Download PDFInfo
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
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- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
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- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
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- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
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- C08G59/68—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the catalysts used
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Abstract
The invention discloses an efficient medium-temperature fast-curing epoxy structural adhesive for die assembly and bonding of wind power generation blades and a preparation method thereof. The high-efficiency medium-temperature fast-curing epoxy structural adhesive mainly comprises a main agent component prepared from a paste epoxy resin mixture and a curing agent component composed of a paste amine mixture. The invention also discloses a preparation method of the composition. The product of the invention combines excellent rigidity, toughness and bonding strength, maintains the operation time of the existing product, shortens the medium-temperature curing period to 2 hours, can help manufacturers to greatly shorten the blade forming period by about 25-30%, accelerates the manufacturing of large blades to within 18 hours, realizes cost reduction in a synergistic manner, and accords with the development trend of the future wind power industry.
Description
Technical Field
The invention belongs to the technical field of epoxy structure preparation, and particularly relates to efficient medium-temperature fast-curing epoxy structure adhesive for die assembly and bonding of wind power generation blades and a preparation method thereof.
Background
The wind energy is a renewable green energy source with great resource potential and mature technology. The development and utilization of wind energy resources can reduce the emission of greenhouse gases, relieve environmental pollution and deal with the effective measures of climate change, and have important significance for the sustainable development of human society. At present, wind power generation is more and more emphasized by countries in the world as clean energy, and is developed and utilized on a large scale in the world.
Driven by a high subsidy policy, the wind power industry in China is in a high-speed growth cycle, the newly added wind power hoisting capacity in China in 2019 is as high as 28.9GW, and the wind power hauler is a global undisputable wind power retriever. However, based on the existing planning, the wind power subsidy is gradually moving back to the slope, and the flat-price internet surfing is realized in 2020.
Therefore, the cost is reduced through technical innovation, the dependence on policy subsidies is eliminated, and the method is a necessary way for future development of the wind power industry.
The manufacturing cost of the wind driven generator blade accounts for about 15% -20% of the whole unit. In the production and manufacturing activities of the blade, along with the improvement of manufacturing materials and the optimization of manufacturing processes, the forming period of the blade is shortened to within 24 hours at present, and the production efficiency is gradually improved.
As a key material for blade production, the heating and curing cycle of the blade structure adhesive is over 5 hours, which accounts for most of the time for wind power blade molding. Therefore, how to shorten the time for closing and bonding the blades is the key for improving the production efficiency and realizing cost reduction and efficiency improvement.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the efficient intermediate-temperature fast-curing epoxy structural adhesive for die assembly and bonding of the wind power generation blade. The structural adhesive maintains the operation time of the existing product, shortens the medium-temperature curing period to 2 hours, helps manufacturers to greatly shorten the blade forming period by about 25-30%, realizes the effects enhancement and cost reduction, and meets the development trend of the future wind power industry.
The invention also aims to provide a preparation method of the high-efficiency intermediate-temperature fast-curing epoxy structural adhesive for die assembly and bonding of the wind power generation blade. In order to achieve one of the purposes of the invention, the following technical scheme is adopted:
an efficient intermediate-temperature fast-curing epoxy structural adhesive for die assembly and bonding of wind power generation blades is composed of a main agent component and a curing agent component.
The main agent component is prepared from the following raw materials in percentage by mass:
the curing agent component is prepared from the following raw materials in percentage by mass:
in a preferred embodiment of the invention, the main agent component is yellow paste, the curing agent component is blue paste, and the mixture is light green paste after being mixed according to the volume ratio of 2:1, and the curing condition is 70 ℃ for 2 hours.
In a preferred embodiment of the invention, the epoxy resin in the main agent component is a mixture of multifunctional epoxy resin and bisphenol A epoxy resin, and the mass mixing ratio is 1: 12.
The multifunctional epoxy resin is one or more of four-functional epoxy resin AG-80 or three-functional epoxy resin AFG-90.
The bisphenol A epoxy resin is one or more of methyl epichlorohydrin bisphenol A epoxy resin or epichlorohydrin bisphenol A epoxy resin.
In a preferred embodiment of the invention, the diluent in the main component is a mixture of a trifunctional epoxy diluent, a difunctional epoxy diluent and a monofunctional epoxy diluent, and the mass mixing ratio is 5:15:1
The monofunctional epoxy diluent is a monofunctional epoxy diluent with a benzene ring.
In a preferred embodiment of the invention, the toughening agent is a mixture of a nitrile rubber-like characteristic polymer capable of forming a sea-island structure and core-shell particles, the mass ratio of the nitrile rubber-like characteristic polymer capable of forming a sea-island structure to the core-shell particles is 5:1, and the nitrile rubber-like characteristic polymer capable of forming a sea-island structure is a Qishi toughening agent;
the core-shell particles are a core-shell structure copolymer with organosilicone rubber as a core and polyacrylate as a shell, and are milky elastic powder in appearance.
In a preferred embodiment of the invention, the first or second functional filler in the main agent component is a mixture of chopped fibers, nano calcium carbonate, nano silica and montmorillonite, and the mass mixing ratio is 1:15:8: 6.
The particle size of the chopped fiber is 20-1500 meshes.
The particle size of the nano silicon dioxide is 300-5000 meshes, and the nano silicon dioxide presents a spherical structure.
The montmorillonite is an organically modified montmorillonite sheet layer, and the particle size is 300-3000 meshes.
In a preferred embodiment of the invention, the amine curing agent in the curing agent component is a mixture of polyether amine, aromatic amine, alicyclic amine, polyamide and a latent curing agent, and the mass mixing ratio is 40:2:3:10: 10.
The latent curing agent is a heat-sensitive blocking curing agent.
In a preferred embodiment of the invention, the latency promoter is a heat-sensitive blocking promoter.
In a preferred embodiment of the invention, the latency promoter is a heat-sensitive blocking promoter. In a preferred embodiment of the invention, the first auxiliary agent is a coupling agent, an antioxidant, a mildew preventive and a pigment, and the mass ratio of the coupling agent to the antioxidant to the mildew preventive is 20:2:3: 0.1.
In a preferred embodiment of the invention, the second auxiliary agent is a coupling agent, an antioxidant, a mildew preventive and a pigment, and the mass ratio of the coupling agent to the antioxidant to the mildew preventive is 10:2:1: 0.1.
In a preferred embodiment of the invention, the hydrophobic thixotropic agent is hydrophobic fumed silica.
In order to realize the second purpose of the invention, the adopted technical scheme is as follows:
a preparation method of efficient intermediate-temperature fast-curing epoxy structural adhesive for die assembly and bonding of wind power generation blades comprises the following steps:
the preparation method of the main agent comprises the following steps:
1) sequentially adding the epoxy resin, the diluent and the toughening agent into a high-speed dispersion kettle according to a proportion, heating to 80-120 ℃, and rapidly stirring and uniformly mixing;
2) cooling to 60-100 ℃, adding the antioxidant, the pigment and the mildew preventive in the first auxiliary agent, and uniformly mixing; adding the first functional filler to disperse uniformly at a high speed;
3) adding the hydrophobic thixotropic agent into the mixture, uniformly stirring, maintaining the temperature, and dispersing at a high speed for 3-5 hours (the rotating speed is 2000-3000 r/min) in a vacuum environment;
4) adding a coupling agent in the first auxiliary agent, stirring for 1-3 hours, filtering and packaging to obtain a main agent component for later use;
the preparation steps of the curing agent are as follows:
1) adding the amine curing agent into a high-speed dispersion kettle, adding the antioxidant, the pigment and the mildew preventive in the second auxiliary agent, and uniformly dispersing at a high speed;
2) continuously adding the second functional filler to uniformly disperse at a high speed; adding a hydrophobic thixotropic agent, uniformly stirring, heating to 60-100 ℃, and dispersing at a high speed for 1-5 hours (the rotating speed is 2000-3000 r/min);
3) and adding a coupling agent in the second auxiliary agent, stirring for 1-3 hours, filtering and packaging to obtain the curing agent component for later use.
The invention has the beneficial effects that:
1) the epoxy resin adopted by the invention is the mixture of multifunctional epoxy resin and bisphenol A epoxy resin, and the combination of the rigidity and the toughness of the structural adhesive is ensured on the molecular structure.
2) The toughening agent adopted by the invention is a mixture of a nitrile rubber-like characteristic polymer capable of forming a sea-island structure and core-shell particles, and achieves the effect of combining rigidity and flexibility on the basis of improving toughness.
3) The amine curing agent adopted by the invention is a mixture of polyether amine, polyamide, alicyclic amine and aromatic amine, the combination of the rigidity and the toughness of the structural adhesive is ensured on the molecular structure, and the long operation time is maintained.
4) The latent curing agent adopted by the invention is a heat-sensitive sealing curing agent, and the latent accelerator is a heat-sensitive sealing accelerator, so that the latent curing agent is stable in the normal-temperature sizing process, and the longer operation time of the product is ensured; the reaction efficiency is rapidly improved in medium-temperature curing, the glass transition temperature reaches 70 ℃ within 2 hours at 70 ℃, and meanwhile, a lower exothermic peak of a system in the heating curing process is kept, so that the aims of enhancing the effect and reducing the cost are fulfilled.
5) The functional filler adopted by the invention is a mixture of chopped fibers, nano calcium carbonate, nano silicon dioxide and montmorillonite, so that the strength, hardness and humidity resistance of the product are improved.
6) The auxiliary agent is mainly a mixture of a coupling agent, an antioxidant and a mildew preventive, improves the stability of storage and bonding, and realizes the shelf life of more than 2 years.
Detailed Description
In order to further explain the high-efficiency intermediate-temperature fast-curing epoxy structural adhesive for die-closing bonding of the wind power generation blade, the preparation methods of a comparative example (a product mature in early period of the company, product number: WD3135D/3137D such as patent CN106753134A, curing condition 70 ℃ for 5 hours) and an example (curing condition 70 ℃ for 2 hours) and the preparation methods of the example (curing condition 70 ℃) are respectively adopted, and the actual performance conditions of the invention are analyzed through physical and chemical properties (glass transition temperature), mechanical properties (body tensile property, impact property, tensile and shearing property), and technological properties (cracking resistance condition and operation time). The scope of the invention is not limited by the following examples.
Example 1:
the main agent, the curing agent, the physical and chemical properties, the mechanical properties and the process properties of the high-efficiency medium-temperature fast-curing epoxy structural adhesive for die assembly and adhesion of the wind power generation blade in the embodiment are shown in table 1:
TABLE 1
The main agent comprises the following components:
the epoxy resin is a mixture of polyfunctional epoxy resin and bisphenol A epoxy resin, and the mixing mass ratio is 1: 12.
The multifunctional epoxy resin is a mixture of four-functional epoxy resin AG-80 and three-functional epoxy resin AFG-90, and the mixing mass ratio is 1: 1.
The bisphenol A epoxy resin is a mixture of methyl epichlorohydrin bisphenol A epoxy resin and epichlorohydrin bisphenol A epoxy resin, and the mixing mass ratio is 1: 3.
The epoxy diluent is a mixture of 636, 622 and CGE, and the mixing mass ratio is 5:15: 1.
The toughening agent is a Qishi toughening agent and core-shell particles, and the mixing mass ratio is 5: 1.
The first or second functional filler is a mixture of chopped fibers, nano calcium carbonate, nano silicon dioxide and montmorillonite, and the mass mixing ratio is 1:15:8: 6.
The auxiliary agents in the main agent component are a coupling agent, an antioxidant, a mildew preventive and a pigment, and the mass ratio of the coupling agent to the antioxidant to the mildew preventive is 20:2:3: 0.1.
The amine curing agent in the curing agent is a mixture of polyether amine, aromatic amine, alicyclic amine, polyamide and latent curing agent, and the mixing mass ratio is 40:2:3:10: 10.
The auxiliary agents in the curing agent component are a coupling agent, an antioxidant, a mildew preventive and a pigment, and the mass ratio of the coupling agent to the antioxidant to the mildew preventive is 10:2:1: 0.1.
Preparation method of efficient medium-temperature fast-curing epoxy structural adhesive for die assembly and bonding of wind power generation blades
1) The preparation method of the main agent comprises the following steps:
sequentially adding the epoxy resin, the diluent and the toughening agent into a high-speed dispersion kettle in proportion through a metering pump, heating to 80-120 ℃, and rapidly stirring and uniformly mixing; cooling to 60-100 ℃, adding the antioxidant, the pigment and the mildew preventive in the first auxiliary agent, and uniformly mixing; adding the first functional filler to disperse uniformly at a high speed;
adding the hydrophobic thixotropic agent, uniformly stirring, maintaining the temperature, and dispersing at a high speed for 3-5 hours in a vacuum environment; adding a coupling agent in the first auxiliary agent, stirring for 1-3 hours, filtering and packaging to obtain a main agent yellow paste colloid;
2) the preparation steps of the curing agent are as follows:
adding an amine curing agent into a high-speed dispersion kettle through a metering pump, adding an antioxidant, a pigment and a mildew preventive in a second auxiliary agent, and uniformly dispersing at a high speed; continuously adding a second functional filler to uniformly disperse at a high speed; adding hydrophobic thixotropic agent, stirring uniformly, heating to 60-100 ℃, and dispersing at high speed for 1-5 hours in the environment; and adding a coupling agent in the second auxiliary agent in a counted amount, stirring for 1-3 hours, filtering and packaging to obtain the curing agent blue paste colloid.
Example 2:
the main agent, the curing agent, the physical and chemical properties, the mechanical properties and the process properties of the high-efficiency medium-temperature fast-curing epoxy structural adhesive for die assembly and adhesion of the wind power generation blade in the embodiment are shown in the table 2:
TABLE 2
The main agent comprises the following components:
the epoxy resin is a mixture of polyfunctional epoxy resin and bisphenol A epoxy resin, and the mixing mass ratio is 1: 5.5.
The multifunctional epoxy resin is a mixture of four-functional epoxy resin AG-80 and three-functional epoxy resin AFG-90, and the mixing mass ratio is 1: 1.
The bisphenol A epoxy resin is a mixture of methyl epichlorohydrin bisphenol A epoxy resin and epichlorohydrin bisphenol A epoxy resin, and the mixing mass ratio is 1: 3.
The epoxy diluent is a mixture of 636, 622 and CGE, and the mixing mass ratio is 5:15: 1.
The toughening agent is a Qishi toughening agent and core-shell particles, and the mixing mass ratio is 5: 1.
The first or second functional filler is a mixture of chopped fibers, nano calcium carbonate, nano silicon dioxide and montmorillonite, and the mass mixing ratio is 1:15:8: 6.
The auxiliary agents in the main agent component are a coupling agent, an antioxidant, a mildew preventive and a pigment, and the mass ratio of the coupling agent to the antioxidant to the mildew preventive is 20:2:3: 0.1.
The amine curing agent in the curing agent is a mixture of polyether amine, aromatic amine, alicyclic amine, polyamide and latent curing agent, and the mixing mass ratio is 40:2:3:10: 10.
The auxiliary agents in the curing agent component are a coupling agent, an antioxidant, a mildew preventive and a pigment, and the mass ratio of the coupling agent to the antioxidant to the mildew preventive is 10:2:1: 0.1.
Preparation method of efficient medium-temperature fast-curing epoxy structural adhesive for die assembly and bonding of wind power generation blades
1) The preparation method of the main agent comprises the following steps:
sequentially adding the epoxy resin, the diluent and the toughening agent into a high-speed dispersion kettle in proportion through a metering pump, heating to 80-120 ℃, and rapidly stirring and uniformly mixing; cooling to 60-100 ℃, adding the antioxidant, the pigment and the mildew preventive in the first auxiliary agent, and uniformly mixing; adding the first functional filler to disperse uniformly at a high speed;
adding the hydrophobic thixotropic agent, uniformly stirring, maintaining the temperature, and dispersing at a high speed for 3-5 hours in a vacuum environment; adding a coupling agent in the first auxiliary agent, stirring for 1-3 hours, filtering and packaging to obtain a main agent yellow paste colloid;
2) the preparation steps of the curing agent are as follows:
adding an amine curing agent into a high-speed dispersion kettle through a metering pump, adding an antioxidant, a pigment and a mildew preventive in a second auxiliary agent, and uniformly dispersing at a high speed; continuously adding a second functional filler to uniformly disperse at a high speed; adding hydrophobic thixotropic agent, stirring uniformly, heating to 60-100 ℃, and dispersing at high speed for 1-5 hours in the environment; and adding a coupling agent in the second auxiliary agent in a counted amount, stirring for 1-3 hours, filtering and packaging to obtain the curing agent blue paste colloid.
Example 3:
the main agent, the curing agent, the physical and chemical properties, the mechanical properties and the process properties of the high-efficiency medium-temperature fast-curing epoxy structural adhesive for die assembly and adhesion of the wind power generation blade in the embodiment are shown in Table 3:
TABLE 3
The main agent comprises the following components:
the bisphenol A epoxy resin is a mixture of methyl epichlorohydrin bisphenol A epoxy resin and epichlorohydrin bisphenol A epoxy resin, and the mixing mass ratio is 1: 3.
The epoxy diluent is a mixture of 636, 622 and CGE, and the mixing mass ratio is 5:15: 1.
The toughening agent is a Qishi toughening agent and core-shell particles, and the mixing mass ratio is 5: 1.
The first or second functional filler is a mixture of chopped fibers, nano calcium carbonate, nano silicon dioxide and montmorillonite, and the mass mixing ratio is 1:15:8: 6.
The auxiliary agents in the main agent component are a coupling agent, an antioxidant, a mildew preventive and a pigment, and the mass ratio of the coupling agent to the antioxidant to the mildew preventive is 20:2:3: 0.1.
The amine curing agent in the curing agent is a mixture of polyether amine, aromatic amine, alicyclic amine, polyamide and latent curing agent, and the mixing mass ratio is 40:2:3:10: 10.
The auxiliary agents in the curing agent component are a coupling agent, an antioxidant, a mildew preventive and a pigment, and the mass ratio of the coupling agent to the antioxidant to the mildew preventive is 10:2:1: 0.1.
Preparation method of efficient medium-temperature fast-curing epoxy structural adhesive for die assembly and bonding of wind power generation blades
1) The preparation method of the main agent comprises the following steps:
sequentially adding the epoxy resin, the diluent and the toughening agent into a high-speed dispersion kettle in proportion through a metering pump, heating to 80-120 ℃, and rapidly stirring and uniformly mixing; cooling to 60-100 ℃, adding the antioxidant, the pigment and the mildew preventive in the first auxiliary agent, and uniformly mixing; adding the first functional filler to disperse uniformly at a high speed;
adding the hydrophobic thixotropic agent, uniformly stirring, maintaining the temperature, and dispersing at a high speed for 3-5 hours in a vacuum environment; adding a coupling agent in the first auxiliary agent, stirring for 1-3 hours, filtering and packaging to obtain a main agent yellow paste colloid;
2) the preparation steps of the curing agent are as follows:
adding an amine curing agent into a high-speed dispersion kettle through a metering pump, adding an antioxidant, a pigment and a mildew preventive in a second auxiliary agent, and uniformly dispersing at a high speed; continuously adding a second functional filler to uniformly disperse at a high speed; adding hydrophobic thixotropic agent, stirring uniformly, heating to 60-100 ℃, and dispersing at high speed for 1-5 hours in the environment; and adding a coupling agent in the second auxiliary agent in a counted amount, stirring for 1-3 hours, filtering and packaging to obtain the curing agent blue paste colloid.
Example 4:
the main agent, the curing agent, the physical and chemical properties, the mechanical properties and the process properties of the high-efficiency medium-temperature fast-curing epoxy structural adhesive for die assembly and adhesion of the wind power generation blade in the embodiment are shown in the table 4:
TABLE 4
The main agent comprises the following components:
the epoxy resin is a mixture of polyfunctional epoxy resin and bisphenol A epoxy resin, and the mixing mass ratio is 1: 12.
The multifunctional epoxy resin is a mixture of four-functional epoxy resin AG-80 and three-functional epoxy resin AFG-90, and the mixing mass ratio is 1: 1.
The bisphenol A epoxy resin is a mixture of methyl epichlorohydrin bisphenol A epoxy resin and epichlorohydrin bisphenol A epoxy resin, and the mixing mass ratio is 1: 3.
The epoxy diluent is a mixture of 636, 622 and CGE, and the mixing mass ratio is 5:15: 1.
The toughening agent is a Qishi toughening agent and core-shell particles, and the mixing mass ratio is 5: 1.
The first or second functional filler is a mixture of chopped fibers, nano calcium carbonate, nano silicon dioxide and montmorillonite, and the mass mixing ratio is 1:15:8: 6.
The auxiliary agents in the main agent component are a coupling agent, an antioxidant, a mildew preventive and a pigment, and the mass ratio of the coupling agent to the antioxidant to the mildew preventive is 20:2:3: 0.1.
The amine curing agent in the curing agent is a mixture of polyether amine, alicyclic amine and a latent curing agent, and the mixing mass ratio is 52:3: 10.
The auxiliary agents in the curing agent component are a coupling agent, an antioxidant, a mildew preventive and a pigment, and the mass ratio of the coupling agent to the antioxidant to the mildew preventive is 10:2:1: 0.1.
Preparation method of efficient medium-temperature fast-curing epoxy structural adhesive for die assembly and bonding of wind power generation blades
1) The preparation method of the main agent comprises the following steps:
sequentially adding the epoxy resin, the diluent and the toughening agent into a high-speed dispersion kettle in proportion through a metering pump, heating to 80-120 ℃, and rapidly stirring and uniformly mixing; cooling to 60-100 ℃, adding the antioxidant, the pigment and the mildew preventive in the first auxiliary agent, and uniformly mixing; adding the first functional filler to disperse uniformly at a high speed;
adding the hydrophobic thixotropic agent, uniformly stirring, maintaining the temperature, and dispersing at a high speed for 3-5 hours in a vacuum environment; adding a coupling agent in the first auxiliary agent, stirring for 1-3 hours, filtering and packaging to obtain a main agent yellow paste colloid;
2) the preparation steps of the curing agent are as follows:
adding an amine curing agent into a high-speed dispersion kettle through a metering pump, adding an antioxidant, a pigment and a mildew preventive in a second auxiliary agent, and uniformly dispersing at a high speed; continuously adding a second functional filler to uniformly disperse at a high speed; adding hydrophobic thixotropic agent, stirring uniformly, heating to 60-100 ℃, and dispersing at high speed for 1-5 hours in the environment; and adding a coupling agent in the second auxiliary agent in a counted amount, stirring for 1-3 hours, filtering and packaging to obtain the curing agent blue paste colloid.
Example 5:
the main agent, the curing agent, the physical and chemical properties, the mechanical properties and the process properties of the high-efficiency medium-temperature fast-curing epoxy structural adhesive for die assembly and adhesion of the wind power generation blade in the embodiment are shown in the table 5:
TABLE 5
The main agent comprises the following components:
the epoxy resin is a mixture of polyfunctional epoxy resin and bisphenol A epoxy resin, and the mixing mass ratio is 1: 12.
The multifunctional epoxy resin is a mixture of four-functional epoxy resin AG-80 and three-functional epoxy resin AFG-90, and the mixing mass ratio is 1: 1.
The bisphenol A epoxy resin is a mixture of methyl epichlorohydrin bisphenol A epoxy resin and epichlorohydrin bisphenol A epoxy resin, and the mixing mass ratio is 1: 3.
The epoxy diluent is a mixture of 636, 622 and CGE, and the mixing mass ratio is 5:15: 1.
The toughening agent is a Qishi toughening agent and core-shell particles, and the mixing mass ratio is 5: 1.
The first or second functional filler is a mixture of chopped fibers, nano calcium carbonate, nano silicon dioxide and montmorillonite, and the mass mixing ratio is 1:15:8: 6.
The auxiliary agents in the main agent component are a coupling agent, an antioxidant, a mildew preventive and a pigment, and the mass ratio of the coupling agent to the antioxidant to the mildew preventive is 20:2:3: 0.1.
The amine curing agent in the curing agent is a mixture of polyether amine, aromatic amine, alicyclic amine and latent curing agent, and the mixing mass ratio is 5:2:3: 10.
The auxiliary agents in the curing agent component are a coupling agent, an antioxidant, a mildew preventive and a pigment, and the mass ratio of the coupling agent to the antioxidant to the mildew preventive is 10:2:1: 0.1.
Preparation method of efficient medium-temperature fast-curing epoxy structural adhesive for die assembly and bonding of wind power generation blades
1) The preparation method of the main agent comprises the following steps:
sequentially adding the epoxy resin, the diluent and the toughening agent into a high-speed dispersion kettle in proportion through a metering pump, heating to 80-120 ℃, and rapidly stirring and uniformly mixing; cooling to 60-100 ℃, adding the antioxidant, the pigment and the mildew preventive in the first auxiliary agent, and uniformly mixing; adding the first functional filler to disperse uniformly at a high speed;
adding the hydrophobic thixotropic agent, uniformly stirring, maintaining the temperature, and dispersing at a high speed for 3-5 hours in a vacuum environment; adding a coupling agent in the first auxiliary agent, stirring for 1-3 hours, filtering and packaging to obtain a main agent yellow paste colloid;
2) the preparation steps of the curing agent are as follows:
adding an amine curing agent into a high-speed dispersion kettle through a metering pump, adding an antioxidant, a pigment and a mildew preventive in a second auxiliary agent, and uniformly dispersing at a high speed; continuously adding a second functional filler to uniformly disperse at a high speed; adding hydrophobic thixotropic agent, stirring uniformly, heating to 60-100 ℃, and dispersing at high speed for 1-5 hours in the environment; and adding a coupling agent in the second auxiliary agent in a counted amount, stirring for 1-3 hours, filtering and packaging to obtain the curing agent blue paste colloid.
Comparative example 1:
the main agent, the curing agent, the physical and chemical properties, the mechanical properties and the process properties of the medium-temperature curing epoxy structural adhesive for die assembly and bonding of the wind power generation blade in the comparative example are shown in Table 6:
TABLE 6
The main agent comprises the following components:
the epoxy resin is a mixture of polyfunctional epoxy resin and bisphenol A epoxy resin, and the mixing mass ratio is 1: 12.
The multifunctional epoxy resin is tetrafunctional epoxy resin AG-80.
The bisphenol A epoxy resin is a mixture of methyl epichlorohydrin bisphenol A epoxy resin and epichlorohydrin bisphenol A epoxy resin, and the mixing mass ratio is 1: 3.
The epoxy diluent is a mixture of 636, 622 and CGE, and the mixing mass ratio is 16:4: 1.
The toughening agent is a Qishi toughening agent and core-shell particles, and the mixing mass ratio is 5: 1.
The first or second functional filler is a mixture of chopped fibers, nano calcium carbonate, nano silicon dioxide and pure magnesium silicate, and the mass mixing ratio is 1:10:20: 6.
The auxiliary agent A is a coupling agent, an antioxidant, a mildew preventive and a molecular sieve, and the mass ratio of the coupling agent to the antioxidant to the mildew preventive to the molecular sieve is 20:2:3: 30.
The amine curing agent in the curing agent is a mixture of polyether amine, aromatic amine, alicyclic amine and polyamide, and the mixing mass ratio is 40:7:3: 15.
The auxiliary agent B is a coupling agent, an antioxidant, a mildew preventive and a molecular sieve, and the mass ratio of the coupling agent to the antioxidant to the mildew preventive to the molecular sieve is 20:2:3: 30.
The specific preparation method is shown in the patent: the yao is superior to the yao, and the Lida is a compound die bonding epoxy structural adhesive for a smog-resistant, damp-heat-resistant wind power generation blade and a preparation method CN106753134A thereof.
Claims (11)
1. The efficient intermediate-temperature fast-curing epoxy structural adhesive for die assembly and bonding of the wind power generation blades is composed of a main agent component and a curing agent component, and is characterized in that the main agent component is prepared from the following raw materials in percentage by mass:
the curing agent component is prepared from the following raw materials in percentage by mass:
2. the efficient intermediate-temperature fast-curing epoxy structural adhesive for die assembly and adhesion of the wind power generation blades as claimed in claim 1, wherein the main agent component is yellow paste, the curing agent component is blue paste, the main agent component and the curing agent component are light green paste after being mixed according to a volume ratio of 2:1, and the curing condition is 70 ℃ and 2 hours.
3. The efficient intermediate-temperature fast-curing epoxy structural adhesive for die assembly and adhesion of the wind power generation blade as claimed in claim 1, wherein the epoxy resin in the main agent component is a mixture of multifunctional epoxy resin and bisphenol A epoxy resin, and the mass mixing ratio is 1: 12.
4. The efficient intermediate-temperature fast-curing epoxy structural adhesive for die assembly and adhesion of the wind power generation blades as claimed in claim 1, wherein the diluent in the main agent component is a mixture of a trifunctional epoxy diluent, a difunctional epoxy diluent and a monofunctional epoxy diluent, and the mass mixing ratio is 5:15: 1.
5. The high-efficiency medium-temperature fast-curing epoxy structural adhesive for die assembly and adhesion of wind power generation blades as claimed in claim 1, wherein the toughening agent is a mixture of a nitrile rubber-like characteristic polymer capable of forming a sea-island structure and core-shell particles, the mass ratio of the nitrile rubber-like characteristic polymer capable of forming a sea-island structure to the core-shell particles is 5:1, and the nitrile rubber-like characteristic polymer capable of forming a sea-island structure is a Qishi toughening agent;
the core-shell particles are a core-shell structure copolymer taking organic silicon-oxygen rubber as a core and polyacrylic ester as a shell, and are milky elastic powder in appearance.
6. The efficient intermediate-temperature fast-curing epoxy structural adhesive for die assembly and adhesion of wind power generation blades as claimed in claim 1, wherein the first or second functional filler in the main agent component is a mixture of chopped fibers, nano calcium carbonate, nano silica and montmorillonite, and the mass mixing ratio is 1:15:8: 6.
7. The efficient intermediate-temperature fast-curing epoxy structural adhesive for die assembly and adhesion of wind power generation blades as claimed in claim 1, wherein the amine curing agent in the curing agent component is a mixture of polyetheramine, aromatic amine, alicyclic amine, polyamide and latent curing agent, and the mass mixing ratio is 40:2:3:10: 10;
the latent curing agent is a heat-sensitive blocking curing agent.
8. The high-efficiency medium-temperature fast-curing epoxy structural adhesive for die assembly and adhesion of wind power generation blades as claimed in claim 1, wherein the latent accelerator is a heat-sensitive sealing accelerator.
9. The efficient intermediate-temperature fast-curing epoxy structural adhesive for die assembly and adhesion of the wind power generation blade as claimed in claim 1, wherein the first auxiliary agent is a coupling agent, an antioxidant, a mildew preventive and a pigment, and the mass ratio of the coupling agent to the antioxidant to the mildew preventive is 20:2:3: 0.1.
The second auxiliary agent is a coupling agent, an antioxidant, a mildew preventive and a pigment, and the mass ratio of the coupling agent to the antioxidant to the mildew preventive to the pigment is 10:2:1: 0.1.
10. The efficient intermediate-temperature fast-curing epoxy structural adhesive for die assembly bonding of wind power generation blades as claimed in claim 1, wherein the hydrophobic thixotropic agent is hydrophobic fumed silica.
11. The preparation method of the high-efficiency intermediate-temperature fast-curing epoxy structural adhesive for die assembly and bonding of the wind power generation blade as claimed in any one of claims 1 to 9, characterized by comprising the following steps:
the preparation method of the main agent comprises the following steps:
1) sequentially adding the epoxy resin, the diluent and the toughening agent into a high-speed dispersion kettle according to a proportion, heating to 80-120 ℃, and rapidly stirring and uniformly mixing;
2) cooling to 60-100 ℃, adding the antioxidant, the pigment and the mildew preventive in the first auxiliary agent, and uniformly mixing; adding the first functional filler to disperse uniformly at a high speed;
3) adding the hydrophobic thixotropic agent into the mixture, uniformly stirring, maintaining the temperature, and dispersing at a high speed for 3-5 hours (the rotating speed is 2000-3000 r/min) in a vacuum environment;
4) adding a coupling agent in the first auxiliary agent, stirring for 1-3 hours, filtering and packaging to obtain a main agent component for later use;
the preparation steps of the curing agent are as follows:
1) adding the amine curing agent into a high-speed dispersion kettle, adding the antioxidant, the pigment and the mildew preventive in the second auxiliary agent, and uniformly dispersing at a high speed;
2) continuously adding the second functional filler to uniformly disperse at a high speed; adding a hydrophobic thixotropic agent, uniformly stirring, heating to 60-100 ℃, and dispersing at a high speed for 1-5 hours (the rotating speed is 2000-3000 r/min);
3) and adding a coupling agent in the second auxiliary agent, stirring for 1-3 hours, filtering and packaging to obtain the curing agent component for later use.
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| CN117511478A (en) * | 2023-11-20 | 2024-02-06 | 重庆胜科检测技术有限公司 | High-toughness epoxy structural adhesive and preparation method thereof |
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